Download citation
Download citation
link to html
In the title compound, (C4H15N3)[UO2(C33H30O5)]·2CH3OH·H2O, the uranyl ion is bound to the four phenoxide groups of the deprotonated p-methyl­dihomooxacalix[4]arene in the usual cone conformation, giving a dianionic complex. The diprotonated diethyl­enetriamine counter-ion links neighbouring complex anions along the b axis through hydrogen bonding with the oxo, phenoxide and ether groups. The solvent mol­ecules are also involved in hydrogen bonding.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806051580/dn2099sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806051580/dn2099Isup2.hkl
Contains datablock I

CCDC reference: 633674

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.024
  • wR factor = 0.059
  • Data-to-parameter ratio = 15.6

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O10 - H10B ... ?
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1 ... ? PLAT480_ALERT_4_C Long H...A H-Bond Reported H3C .. O6 .. 2.61 Ang.
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: HKL-2000 (Otwinowski & Minor, 1997); data reduction: HKL-2000; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1999); software used to prepare material for publication: SHELXTL (Bruker, 1999) and PLATON (Spek, 2003).

diethylenetriamine(2+) (p-methyldihomooxacalix[4]arene)dioxouranium methanol disolvate monohydrate top
Crystal data top
(C4H15N3)[UO2(C33H30O5)]·2CH4O·H2OF(000) = 1928
Mr = 963.89Dx = 1.609 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 131799 reflections
a = 11.9895 (4) Åθ = 2.2–25.7°
b = 16.2079 (3) ŵ = 4.14 mm1
c = 21.2475 (6) ÅT = 100 K
β = 105.441 (2)°Platelet, translucent light orange
V = 3979.88 (19) Å30.21 × 0.15 × 0.07 mm
Z = 4
Data collection top
Nonius KappaCCD area-detector
diffractometer
7565 independent reflections
Radiation source: fine-focus sealed tube6173 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.029
two φ and four ω scans with 2° stepsθmax = 25.7°, θmin = 2.2°
Absorption correction: multi-scan
(SCALEPACK; Otwinowski & Minor, 1997)
h = 1414
Tmin = 0.528, Tmax = 0.749k = 1919
131799 measured reflectionsl = 2525
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.059H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0321P)2]
where P = (Fo2 + 2Fc2)/3
7565 reflections(Δ/σ)max = 0.001
484 parametersΔρmax = 0.51 e Å3
0 restraintsΔρmin = 1.00 e Å3
Special details top

Experimental. crystal-to-detector distance 30 mm

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms bound to N and O atoms were found on a Fourier-difference map and all the others were introduced at calculated positions. All were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (NH, OH, CH, CH2) or 1.5 (CH3) times that of the parent atom. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
U10.677598 (9)0.625673 (7)0.187022 (5)0.02124 (5)
O10.76745 (18)0.67694 (12)0.11436 (10)0.0244 (5)
O20.84197 (18)0.55225 (12)0.22779 (10)0.0223 (5)
O30.62669 (18)0.55593 (12)0.26763 (10)0.0235 (5)
O40.49581 (18)0.68030 (12)0.16470 (10)0.0236 (5)
O50.62143 (17)0.82913 (13)0.13096 (10)0.0239 (5)
O60.62086 (18)0.54278 (12)0.13122 (10)0.0258 (5)
O70.73486 (18)0.70749 (12)0.24246 (10)0.0235 (5)
O80.7838 (2)0.61700 (15)0.00367 (12)0.0403 (6)
H80.78030.63460.03430.048*
O90.35380 (19)0.58340 (14)0.07575 (11)0.0334 (5)
H90.39510.61790.09980.040*
O100.5316 (2)0.40786 (14)0.22347 (11)0.0339 (5)
H10A0.55630.45740.24670.041*
H10B0.52630.37780.25500.041*
N10.8569 (2)0.81579 (16)0.38767 (12)0.0257 (6)
H10.83920.76440.37220.031*
N20.7175 (2)0.88604 (15)0.27099 (12)0.0252 (6)
H2A0.69170.86510.23150.030*
H2B0.79200.87920.28380.030*
H2C0.70520.94220.26860.030*
N31.0640 (2)0.91990 (17)0.41588 (13)0.0293 (6)
H3A1.02330.90490.37190.035*
H3B1.12580.89680.41970.035*
H3C1.08370.97800.41640.035*
C10.8010 (3)0.82014 (19)0.10236 (14)0.0223 (7)
C20.8425 (3)0.74063 (18)0.12380 (14)0.0225 (7)
C30.9620 (3)0.72857 (19)0.15209 (14)0.0230 (7)
C41.0362 (3)0.79468 (19)0.15338 (15)0.0267 (7)
H41.11500.78670.17150.032*
C50.9980 (3)0.8724 (2)0.12873 (15)0.0277 (7)
C60.8786 (3)0.88410 (19)0.10475 (15)0.0255 (7)
H60.85060.93610.09000.031*
C71.0807 (3)0.9425 (2)0.12823 (19)0.0374 (8)
H7A1.06330.96640.08540.056*
H7B1.15860.92200.13980.056*
H7C1.07260.98380.15920.056*
C81.0079 (3)0.64416 (19)0.17957 (15)0.0251 (7)
H8A0.95800.60170.15480.030*
H8B1.08450.63640.17330.030*
C91.0149 (3)0.63286 (19)0.25192 (15)0.0241 (7)
C100.9310 (3)0.58834 (19)0.27263 (15)0.0230 (7)
C110.9375 (3)0.58201 (19)0.33982 (15)0.0239 (7)
C121.0329 (3)0.61584 (19)0.38469 (16)0.0286 (7)
H121.03880.61040.42900.034*
C131.1198 (3)0.6576 (2)0.36545 (16)0.0309 (8)
C141.1078 (3)0.6666 (2)0.29893 (16)0.0303 (8)
H141.16360.69610.28530.036*
C151.2258 (3)0.6895 (3)0.41522 (17)0.0434 (10)
H15A1.28400.64730.42490.065*
H15B1.20530.70460.45440.065*
H15C1.25520.73700.39790.065*
C160.8457 (3)0.53629 (19)0.36423 (15)0.0236 (7)
H16A0.81370.49310.33310.028*
H16B0.88400.50960.40510.028*
C170.7455 (3)0.58680 (19)0.37518 (15)0.0228 (7)
C180.6400 (3)0.59314 (18)0.32635 (14)0.0211 (6)
C190.5463 (3)0.63793 (18)0.33831 (15)0.0245 (7)
C200.5603 (3)0.67364 (19)0.39930 (16)0.0272 (7)
H200.49900.70310.40740.033*
C210.6633 (3)0.66700 (19)0.44914 (15)0.0255 (7)
C220.7544 (3)0.62394 (18)0.43542 (15)0.0243 (7)
H220.82390.61980.46770.029*
C230.6756 (3)0.7049 (2)0.51545 (16)0.0343 (8)
H23A0.71990.75490.51910.052*
H23B0.71450.66680.54870.052*
H23C0.60040.71710.52080.052*
C240.4329 (3)0.64648 (19)0.28533 (15)0.0253 (7)
H24A0.42880.60330.25320.030*
H24B0.36910.63840.30470.030*
C250.4187 (3)0.72948 (19)0.25111 (15)0.0233 (7)
C260.4554 (3)0.74287 (19)0.19435 (15)0.0241 (7)
C270.4500 (3)0.82311 (19)0.16759 (15)0.0223 (7)
C280.4046 (3)0.88776 (19)0.19626 (15)0.0254 (7)
H280.40170.94040.17850.031*
C290.3634 (3)0.87514 (19)0.25072 (16)0.0278 (7)
C300.3722 (3)0.79603 (19)0.27682 (15)0.0259 (7)
H300.34540.78710.31350.031*
C310.3158 (3)0.9456 (2)0.28258 (17)0.0336 (8)
H31A0.24390.92920.29060.050*
H31B0.30310.99270.25410.050*
H31C0.37020.95970.32320.050*
C320.4969 (3)0.8365 (2)0.10997 (15)0.0247 (7)
H32A0.46520.79570.07660.030*
H32B0.47540.89090.09170.030*
C330.6730 (3)0.83217 (19)0.07704 (14)0.0234 (7)
H33A0.65700.88510.05510.028*
H33B0.64040.78920.04580.028*
C340.7488 (3)0.85776 (19)0.38811 (15)0.0260 (7)
H34A0.76410.91540.39940.031*
H34B0.71570.83270.42050.031*
C350.6652 (3)0.8507 (2)0.32137 (16)0.0270 (7)
H35A0.64590.79320.31150.032*
H35B0.59440.88010.32080.032*
C360.9432 (3)0.8156 (2)0.45108 (16)0.0302 (8)
H36A1.00160.77420.45100.036*
H36B0.90620.80140.48500.036*
C371.0001 (3)0.8992 (2)0.46540 (15)0.0280 (7)
H37A0.94160.94080.46460.034*
H37B1.05340.89890.50870.034*
C380.8989 (3)0.6298 (3)0.0062 (2)0.0522 (11)
H38A0.92180.68530.00690.078*
H38B0.90410.62090.05000.078*
H38C0.94900.59180.02270.078*
C390.2453 (3)0.5829 (3)0.0899 (2)0.0486 (10)
H39A0.25370.55990.13260.073*
H39B0.19180.55010.05810.073*
H39C0.21670.63830.08890.073*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
U10.02394 (7)0.01933 (7)0.01998 (7)0.00008 (5)0.00504 (5)0.00163 (5)
O10.0246 (11)0.0253 (11)0.0233 (11)0.0018 (9)0.0064 (9)0.0005 (9)
O20.0242 (11)0.0205 (11)0.0215 (11)0.0005 (9)0.0049 (9)0.0019 (9)
O30.0286 (12)0.0210 (11)0.0215 (11)0.0046 (9)0.0078 (9)0.0020 (9)
O40.0234 (11)0.0221 (11)0.0252 (11)0.0028 (9)0.0065 (9)0.0022 (9)
O50.0199 (11)0.0324 (12)0.0186 (11)0.0003 (9)0.0035 (9)0.0020 (9)
O60.0291 (12)0.0219 (11)0.0259 (12)0.0001 (9)0.0067 (10)0.0020 (9)
O70.0279 (12)0.0200 (11)0.0229 (11)0.0008 (9)0.0074 (9)0.0005 (9)
O80.0335 (13)0.0562 (17)0.0299 (13)0.0053 (12)0.0062 (11)0.0113 (12)
O90.0263 (12)0.0367 (13)0.0360 (13)0.0015 (11)0.0062 (10)0.0104 (11)
O100.0474 (15)0.0301 (12)0.0244 (12)0.0093 (11)0.0102 (11)0.0022 (10)
N10.0277 (15)0.0221 (13)0.0262 (14)0.0014 (11)0.0050 (12)0.0003 (11)
N20.0280 (14)0.0234 (14)0.0215 (13)0.0002 (11)0.0018 (11)0.0007 (11)
N30.0271 (15)0.0311 (15)0.0275 (15)0.0010 (12)0.0032 (12)0.0036 (12)
C10.0248 (16)0.0255 (16)0.0174 (15)0.0007 (13)0.0070 (13)0.0017 (12)
C20.0296 (17)0.0210 (15)0.0179 (15)0.0004 (13)0.0077 (13)0.0014 (12)
C30.0249 (16)0.0270 (17)0.0178 (15)0.0002 (13)0.0069 (13)0.0027 (13)
C40.0265 (17)0.0297 (17)0.0236 (16)0.0045 (14)0.0063 (13)0.0021 (14)
C50.0279 (17)0.0300 (18)0.0261 (16)0.0022 (15)0.0090 (13)0.0038 (14)
C60.0287 (17)0.0244 (16)0.0250 (16)0.0036 (14)0.0102 (13)0.0001 (13)
C70.032 (2)0.0303 (18)0.050 (2)0.0030 (15)0.0116 (17)0.0035 (17)
C80.0235 (16)0.0265 (17)0.0268 (17)0.0063 (13)0.0093 (13)0.0036 (13)
C90.0206 (15)0.0269 (17)0.0247 (16)0.0055 (13)0.0059 (12)0.0003 (13)
C100.0220 (16)0.0204 (15)0.0255 (16)0.0053 (13)0.0043 (13)0.0021 (13)
C110.0243 (16)0.0236 (16)0.0227 (16)0.0045 (13)0.0045 (13)0.0019 (13)
C120.0283 (17)0.0323 (18)0.0233 (16)0.0038 (15)0.0035 (13)0.0014 (14)
C130.0255 (18)0.0401 (19)0.0259 (17)0.0004 (15)0.0050 (14)0.0033 (15)
C140.0236 (17)0.038 (2)0.0307 (18)0.0008 (15)0.0092 (14)0.0008 (15)
C150.031 (2)0.067 (3)0.031 (2)0.0115 (19)0.0063 (16)0.0041 (19)
C160.0271 (17)0.0239 (16)0.0195 (15)0.0020 (14)0.0057 (13)0.0018 (13)
C170.0272 (17)0.0204 (15)0.0232 (16)0.0021 (13)0.0109 (13)0.0030 (13)
C180.0264 (16)0.0171 (14)0.0211 (15)0.0037 (13)0.0087 (13)0.0001 (12)
C190.0293 (17)0.0193 (16)0.0258 (16)0.0050 (13)0.0090 (13)0.0008 (13)
C200.0279 (17)0.0261 (17)0.0304 (17)0.0004 (14)0.0124 (14)0.0013 (14)
C210.0292 (17)0.0246 (17)0.0236 (16)0.0049 (14)0.0086 (14)0.0019 (13)
C220.0261 (16)0.0229 (16)0.0237 (15)0.0031 (14)0.0062 (13)0.0015 (13)
C230.041 (2)0.039 (2)0.0249 (17)0.0006 (17)0.0114 (15)0.0054 (15)
C240.0227 (16)0.0265 (17)0.0281 (17)0.0001 (13)0.0092 (13)0.0004 (13)
C250.0170 (15)0.0269 (16)0.0248 (16)0.0028 (13)0.0032 (13)0.0009 (13)
C260.0179 (15)0.0279 (17)0.0251 (16)0.0012 (13)0.0032 (13)0.0065 (13)
C270.0169 (15)0.0253 (16)0.0226 (15)0.0005 (13)0.0014 (12)0.0014 (13)
C280.0202 (15)0.0246 (17)0.0276 (16)0.0010 (13)0.0004 (13)0.0019 (13)
C290.0224 (16)0.0282 (17)0.0326 (17)0.0019 (14)0.0074 (13)0.0055 (15)
C300.0209 (16)0.0313 (18)0.0261 (16)0.0042 (14)0.0074 (13)0.0033 (14)
C310.0342 (19)0.0320 (19)0.037 (2)0.0040 (15)0.0133 (16)0.0040 (16)
C320.0198 (16)0.0267 (16)0.0240 (16)0.0003 (13)0.0004 (13)0.0010 (13)
C330.0273 (17)0.0259 (16)0.0177 (15)0.0014 (14)0.0073 (13)0.0007 (13)
C340.0298 (17)0.0233 (17)0.0247 (16)0.0014 (13)0.0073 (14)0.0008 (13)
C350.0245 (17)0.0250 (16)0.0326 (18)0.0037 (13)0.0093 (14)0.0019 (14)
C360.0354 (19)0.0250 (17)0.0277 (17)0.0043 (15)0.0042 (14)0.0070 (14)
C370.0277 (17)0.0319 (18)0.0223 (16)0.0003 (14)0.0031 (13)0.0017 (14)
C380.036 (2)0.082 (3)0.039 (2)0.003 (2)0.0098 (17)0.014 (2)
C390.036 (2)0.043 (2)0.070 (3)0.0002 (18)0.021 (2)0.008 (2)
Geometric parameters (Å, º) top
U1—O12.263 (2)C15—H15A0.9600
U1—O22.267 (2)C15—H15B0.9600
U1—O32.267 (2)C15—H15C0.9600
U1—O42.282 (2)C16—C171.521 (4)
U1—O61.801 (2)C16—H16A0.9700
U1—O71.785 (2)C16—H16B0.9700
O1—C21.349 (4)C17—C221.393 (4)
O2—C101.359 (4)C17—C181.410 (4)
O3—C181.356 (3)C18—C191.417 (4)
O4—C261.350 (4)C19—C201.388 (4)
O5—C331.440 (4)C19—C241.523 (4)
O5—C321.445 (4)C20—C211.400 (4)
O8—C381.410 (4)C20—H200.9300
O8—H80.8684C21—C221.391 (4)
O9—C391.411 (4)C21—C231.508 (4)
O9—H90.8273C22—H220.9300
O10—H10A0.9472C23—H23A0.9600
O10—H10B0.8444C23—H23B0.9600
N1—C361.464 (4)C23—H23C0.9600
N1—C341.466 (4)C24—C251.517 (4)
N1—H10.9006C24—H24A0.9700
N2—C351.491 (4)C24—H24B0.9700
N2—H2A0.8813C25—C301.391 (4)
N2—H2B0.8689C25—C261.407 (4)
N2—H2C0.9215C26—C271.414 (4)
N3—C371.496 (4)C27—C281.394 (4)
N3—H3A0.9625C27—C321.493 (4)
N3—H3B0.8148C28—C291.389 (5)
N3—H3C0.9705C28—H280.9300
C1—C61.384 (4)C29—C301.390 (4)
C1—C21.412 (4)C29—C311.515 (4)
C1—C331.498 (4)C30—H300.9300
C2—C31.411 (4)C31—H31A0.9600
C3—C41.388 (4)C31—H31B0.9600
C3—C81.531 (4)C31—H31C0.9600
C4—C51.395 (4)C32—H32A0.9700
C4—H40.9300C32—H32B0.9700
C5—C61.399 (4)C33—H33A0.9700
C5—C71.510 (4)C33—H33B0.9700
C6—H60.9300C34—C351.507 (4)
C7—H7A0.9600C34—H34A0.9700
C7—H7B0.9600C34—H34B0.9700
C7—H7C0.9600C35—H35A0.9700
C8—C91.528 (4)C35—H35B0.9700
C8—H8A0.9700C36—C371.511 (4)
C8—H8B0.9700C36—H36A0.9700
C9—C141.394 (4)C36—H36B0.9700
C9—C101.401 (4)C37—H37A0.9700
C10—C111.412 (4)C37—H37B0.9700
C11—C121.392 (4)C38—H38A0.9600
C11—C161.528 (4)C38—H38B0.9600
C12—C131.392 (5)C38—H38C0.9600
C12—H120.9300C39—H39A0.9600
C13—C141.390 (5)C39—H39B0.9600
C13—C151.511 (5)C39—H39C0.9600
C14—H140.9300
O1—U1—O285.99 (7)C18—C17—C16121.1 (3)
O2—U1—O380.28 (7)O3—C18—C17120.5 (3)
O3—U1—O485.19 (8)O3—C18—C19119.2 (3)
O4—U1—O1108.51 (7)C17—C18—C19120.3 (3)
O6—U1—O7179.58 (10)C20—C19—C18118.5 (3)
O7—U1—O190.47 (8)C20—C19—C24121.0 (3)
O6—U1—O189.41 (9)C18—C19—C24120.6 (3)
O7—U1—O390.31 (8)C19—C20—C21122.5 (3)
O6—U1—O389.71 (8)C19—C20—H20118.8
O1—U1—O3166.25 (8)C21—C20—H20118.8
O7—U1—O289.73 (9)C22—C21—C20117.6 (3)
O6—U1—O289.85 (8)C22—C21—C23120.9 (3)
O7—U1—O491.56 (8)C20—C21—C23121.5 (3)
O6—U1—O488.87 (8)C21—C22—C17122.5 (3)
O2—U1—O4165.42 (8)C21—C22—H22118.7
C2—O1—U1126.84 (18)C17—C22—H22118.7
C10—O2—U1118.84 (17)C21—C23—H23A109.5
C18—O3—U1118.93 (17)C21—C23—H23B109.5
C26—O4—U1129.49 (18)H23A—C23—H23B109.5
C33—O5—C32112.3 (2)C21—C23—H23C109.5
C38—O8—H8106.1H23A—C23—H23C109.5
C39—O9—H9107.8H23B—C23—H23C109.5
H10A—O10—H10B98.9C25—C24—C19113.5 (3)
C36—N1—C34113.9 (3)C25—C24—H24A108.9
C36—N1—H1111.9C19—C24—H24A108.9
C34—N1—H1108.0C25—C24—H24B108.9
C35—N2—H2A115.3C19—C24—H24B108.9
C35—N2—H2B108.6H24A—C24—H24B107.7
H2A—N2—H2B108.7C30—C25—C26117.8 (3)
C35—N2—H2C109.1C30—C25—C24120.3 (3)
H2A—N2—H2C108.6C26—C25—C24121.8 (3)
H2B—N2—H2C106.2O4—C26—C25121.2 (3)
C37—N3—H3A113.8O4—C26—C27119.2 (3)
C37—N3—H3B116.7C25—C26—C27119.7 (3)
H3A—N3—H3B101.2C28—C27—C26119.8 (3)
C37—N3—H3C112.3C28—C27—C32121.7 (3)
H3A—N3—H3C108.4C26—C27—C32118.4 (3)
H3B—N3—H3C103.5C29—C28—C27121.3 (3)
C6—C1—C2119.7 (3)C29—C28—H28119.3
C6—C1—C33122.0 (3)C27—C28—H28119.3
C2—C1—C33118.3 (3)C28—C29—C30117.6 (3)
O1—C2—C3121.2 (3)C28—C29—C31121.4 (3)
O1—C2—C1119.1 (3)C30—C29—C31121.0 (3)
C3—C2—C1119.6 (3)C29—C30—C25123.7 (3)
C4—C3—C2118.3 (3)C29—C30—H30118.2
C4—C3—C8121.2 (3)C25—C30—H30118.2
C2—C3—C8120.5 (3)C29—C31—H31A109.5
C3—C4—C5123.0 (3)C29—C31—H31B109.5
C3—C4—H4118.5H31A—C31—H31B109.5
C5—C4—H4118.5C29—C31—H31C109.5
C4—C5—C6117.5 (3)H31A—C31—H31C109.5
C4—C5—C7122.1 (3)H31B—C31—H31C109.5
C6—C5—C7120.4 (3)O5—C32—C27108.6 (2)
C1—C6—C5121.6 (3)O5—C32—H32A110.0
C1—C6—H6119.2C27—C32—H32A110.0
C5—C6—H6119.2O5—C32—H32B110.0
C5—C7—H7A109.5C27—C32—H32B110.0
C5—C7—H7B109.5H32A—C32—H32B108.3
H7A—C7—H7B109.5O5—C33—C1109.0 (2)
C5—C7—H7C109.5O5—C33—H33A109.9
H7A—C7—H7C109.5C1—C33—H33A109.9
H7B—C7—H7C109.5O5—C33—H33B109.9
C9—C8—C3114.1 (3)C1—C33—H33B109.9
C9—C8—H8A108.7H33A—C33—H33B108.3
C3—C8—H8A108.7N1—C34—C35109.1 (3)
C9—C8—H8B108.7N1—C34—H34A109.9
C3—C8—H8B108.7C35—C34—H34A109.9
H8A—C8—H8B107.6N1—C34—H34B109.9
C14—C9—C10118.7 (3)C35—C34—H34B109.9
C14—C9—C8119.6 (3)H34A—C34—H34B108.3
C10—C9—C8121.7 (3)N2—C35—C34110.2 (3)
O2—C10—C9119.8 (3)N2—C35—H35A109.6
O2—C10—C11119.9 (3)C34—C35—H35A109.6
C9—C10—C11120.2 (3)N2—C35—H35B109.6
C12—C11—C10118.6 (3)C34—C35—H35B109.6
C12—C11—C16119.6 (3)H35A—C35—H35B108.1
C10—C11—C16121.8 (3)N1—C36—C37110.7 (3)
C11—C12—C13122.2 (3)N1—C36—H36A109.5
C11—C12—H12118.9C37—C36—H36A109.5
C13—C12—H12118.9N1—C36—H36B109.5
C14—C13—C12117.8 (3)C37—C36—H36B109.5
C14—C13—C15121.1 (3)H36A—C36—H36B108.1
C12—C13—C15121.1 (3)N3—C37—C36110.4 (3)
C13—C14—C9122.3 (3)N3—C37—H37A109.6
C13—C14—H14118.8C36—C37—H37A109.6
C9—C14—H14118.8N3—C37—H37B109.6
C13—C15—H15A109.5C36—C37—H37B109.6
C13—C15—H15B109.5H37A—C37—H37B108.1
H15A—C15—H15B109.5O8—C38—H38A109.5
C13—C15—H15C109.5O8—C38—H38B109.5
H15A—C15—H15C109.5H38A—C38—H38B109.5
H15B—C15—H15C109.5O8—C38—H38C109.5
C17—C16—C11117.4 (3)H38A—C38—H38C109.5
C17—C16—H16A107.9H38B—C38—H38C109.5
C11—C16—H16A107.9O9—C39—H39A109.5
C17—C16—H16B107.9O9—C39—H39B109.5
C11—C16—H16B107.9H39A—C39—H39B109.5
H16A—C16—H16B107.2O9—C39—H39C109.5
C22—C17—C18118.6 (3)H39A—C39—H39C109.5
C22—C17—C16120.2 (3)H39B—C39—H39C109.5
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8···O10.871.882.745 (3)177
O9—H9···O40.831.872.688 (3)170
O10—H10A···O30.951.812.715 (3)160
N2—H2B···N10.872.372.834 (4)114
N2—H2A···O70.882.602.975 (3)106
N2—H2A···O50.882.163.034 (3)173
N2—H2C···O2i0.921.882.788 (3)169
N2—H2B···O10i0.872.213.000 (4)151
N3—H3A···N10.962.562.929 (4)103
N3—H3C···O6i0.972.612.950 (3)101
N3—H3B···O8ii0.812.162.797 (4)136
N3—H3C···O9i0.971.852.816 (4)170
N3—H3A···O10i0.961.962.883 (3)160
O10—H10b···Cgiii0.842.673.47160
Symmetry codes: (i) x+3/2, y+1/2, z+1/2; (ii) x+1/2, y+3/2, z+1/2; (iii) x+3/2, y1/2, z+1/2.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds